CN106492657A - A kind of allophane nano-tube hydridization forward osmosis membrane - Google Patents
A kind of allophane nano-tube hydridization forward osmosis membrane Download PDFInfo
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- CN106492657A CN106492657A CN201610847062.5A CN201610847062A CN106492657A CN 106492657 A CN106492657 A CN 106492657A CN 201610847062 A CN201610847062 A CN 201610847062A CN 106492657 A CN106492657 A CN 106492657A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/002—Forward osmosis or direct osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
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Abstract
The invention discloses a kind of allophane nano-tube hydridization forward osmosis membrane, the method is using allophane nano-tube as modifying agent, pre-dispersed in casting solution, by inversion of phases film forming, allophane nano-tube hydridization forward osmosis membrane is obtained in conjunction with interfacial polymerization, the interior concentration polarization of forward osmosis membrane is effectively reduced, the water flux of forward osmosis membrane is improve.Forward osmosis membrane provided by the present invention has high permeating flux and efficient selective.
Description
Technical field
The invention belongs to technical field of membrane separation, and in particular to a kind of allophane nano-tube hydridization forward osmosis membrane.
Background technology
Forward osmosis membrane technology is one of new century most promising separation membrane technology.By taking salt solution as an example, forward osmosis membrane
There is a permeable pressure head because concentration is different in the solution of both sides, permeable pressure head allows the water to the side higher from concentration spontaneously
The relatively low side of concentration is diffused to, and forward osmosis membrane plays a part of to intercept salt ion wherein.Compared to reverse osmosis membrane, nanofiltration
Film and microfiltration membranes, forward osmosis membrane in application process by osmotic pressure as driving force, without the need for impressed pressure, energy-conserving and environment-protective advantage is bright
Aobvious.At present, forward osmosis membrane technology desalinization, environmental protection, petrochemical industry, power-saving technology, clean manufacturing, medicine, food,
Electronic applications have good development prospect.But, the presence of interior concentration polarization has had a strong impact on the practical application of forward osmosis membrane
In performance.Interior concentration polarization is inevitable, and the hydrophily for reducing the structural parameters and raising film of forward osmosis membrane becomes reduction
The effective means of interior concentration polarization.
In eliminating, one of method of concentration polarization is to introduce inorganic material, using the hydrophily of inorganic material itself, improves
The wellability on film surface, improves its permeation flux to a certain extent.Meanwhile, inorganic layer can play the work of physical barriers
With realizing separation function.Common inorganic material has：Nano silicon, nano titanium oxide, Nano Silver, graphene oxide
With CNT etc..
Allophane nano-tube is that a kind of internal diameter is about 1nm, and external diameter is 2～2.5nm, and length is in 100～200nm
Empty nanotube.The chemical formula (OH) of allophane nano-tube3Al2O3SiOH, the outer wall of nanotube exist substantial amounts of with inwall
Hydroxyl, thus allophane nano-tube has high hydrophily.Method using blending and modifying is by allophane silicon nanometer
Pipe is doped in basilar memebrane, is prepared forward osmosis membrane and can be effectively improved porosity, increase permeation flux, so as to reduce the knot of film
Fruit parameter, plays a part of to reduce concentration polarization in forward osmosis membrane.104437134 A of Chinese patent CN locate after disclosing one kind
The modified method for preparing the positive impregnating polyamide composite membrane of high selectivity of reason, is formed using the reaction between polyamine and polynary acyl chlorides
Covalent bond is aggregated on supporting layer, is greatly reduced the solute back-mixing flux of film, is effectively improved the selection performance of film.Although should
Method can be effectively improved the selectivity of forward osmosis membrane, but the complex operation step of the method, while often with the water of expendable film
Flux is cost.By contrast, allophane nano-tube hydridization forward osmosis membrane so which is simple to operate, be easy to the features such as amplifying and
There is bigger practical value, and can keep necessarily selectively not simultaneously, largely improving the permeation flux of film.
Content of the invention
Present invention aims to the deficiencies in the prior art, there is provided a kind of allophane nano-tube hydridization is just oozed
Permeable membrane, the invention are not only simple to operate, and energy effective guarantee allophane nanotube is fixed in forward osmosis membrane matrix, made
The polymer separation film for obtaining has long-acting high flux, selectivity and service life.
The purpose of the present invention is achieved through the following technical solutions：A kind of allophane nano-tube hydridization is just permeated
Film, the allophane nano-tube hydridization forward osmosis membrane are prepared by the following method and obtain：
(1) allophane nano-tube, polymer, decentralized medium are mixed with organic solvent, ultrasonic wave dispersion 5min～
2h, heating stirring form uniform solution；In described casting solution, polymer, allophane nano-tube, the matter of decentralized medium
Amount is than being 10～30:0.01～3:1～4, and the mass percentage concentration of polymer is 15～35%, allophane nano-tube
Mass percentage concentration is 0.1～3%；Described ultrasonic frequency 20KHz～100KHz；Described heating stirring temperature be 40～
80 DEG C, mixing time is 2～12h；
(2) casting solution is obtained after 10～24h of standing and defoaming, make primary membrane by film forming is machining；
(3) submergence 10min～8h in coagulating bath is entered in 5min after primary membrane shaping obtain hydrophilic base film；Described
Coagulating bath is the aqueous solution of deionized water or polar non-solute that weight/mass percentage composition is 10～60%；Described coagulating bath
Temperature is 10～60 DEG C；
(4) further for basilar memebrane interfacial polymerization is formed aramid layer, obtains allophane nano-tube hydridization and just permeate
Film, the step are specially：Basilar memebrane is immersed 0.1min～6min in the aqueous solution of polyamine, unnecessary polyamine is removed water-soluble
Liquid, then 0.1min～6min in the organic solution of polynary acyl chlorides is immersed, remove unnecessary polynary solution of acid chloride；After maturation process,
It is obtained and there is the allophane nano-tube hydridization forward osmosis membrane for cutting salt functional.The mass concentration of described polynary amine aqueous solution is
0.01～1%；In the organic solution of described polynary acyl chlorides, the mass ratio of polynary acyl chlorides and organic solvent is 0.1～1:800～
1000.
Further, described allophane nano-tube is to be closed by sodium orthosilicate and ANN aluminium nitrate nonahydrate by the following method
Into obtained：It is 0.58 by mol ratio:1 sodium orthosilicate and ANN aluminium nitrate nonahydrate are prepared into solution, and concentration is 0.1M hydrogen
Sodium oxide molybdena adjusts the pH value of solution to 4.5～5, reuse concentration for 0.1M hydrochloric acid by the pH of solution to adjusting to 4.3, solution
After standing 2h, 95 DEG C are heated 3～7 days, are stored at room temperature cooling, are that 0.1M ammonium hydroxide adjusts pH value to 8～9 with concentration, are formed
Gel, under 5000～9000rmp is centrifuged 10min～1h, obtains allophane nano-tube.
Further, described polymer by Kynoar, polyacrylonitrile, polysulfones, polyether sulfone, cellulose derivative,
One or more in polyimides, polytetrafluoroethylene (PTFE) is by any proportioning mixing composition；Described decentralized medium by water, ethanol,
One or more in methyl alcohol are by any proportioning mixing composition；Described organic solvent is by dimethyl sulfoxide, N, N- dimethyl formyls
One or more in amine, DMAC N,N' dimethyl acetamide, methyl pyrrolidone is by any proportioning mixing composition.
Further, described coagulating bath is the aqueous solution that weight/mass percentage composition is 10～30% polar non-solutes.
Further, described polyamine is by m-phenylene diamine (MPD), o-phenylenediamine, p-phenylenediamine, equal benzene triamine, piperazine and piperazine
Derivative one or more by any proportioning mixing composition.
Further, described polynary acyl chlorides is by pyromellitic trimethylsilyl chloride, m-phthaloyl chloride, o-phthaloyl chloride and to benzene
In dimethyl chloride, one or more are by any proportioning mixing composition.
Further, the organic solvent in the organic solution of described polynary acyl chlorides by normal heptane, n-hexane, hexamethylene,
One or more in naphthalene, Isopar-G and Isopar-E are by any proportioning mixing composition.
Further, described maturation process is specially：Composite membrane is put into immersion 0.5min～5min in 95 DEG C of water,
It is put into after taking-up in the aqueous sodium hypochlorite solution that mass concentration is 0.1g/L～1g/L and soaks 0.1min～10min, puts after taking-up
Enter in the aqueous sodium hypochlorite solution that mass concentration is 0.1g/L～3g/L and soak 0.5min～10min；95 DEG C are put into after taking-up
Immersion 0.5min～5min or 5min～40min is heated in being put into 60～80 DEG C of baking oven in water.Further, its feature exists
In the polar non-solute is by dimethyl sulfoxide, DMF, DMA, crassitude
One or more in ketone is by any proportioning mixing composition.
The device have the advantages that：The present invention is passed through by being directly added into allophane nano-tube in casting solution
After crossing forming film with phase transformation method, allophane nano-tube is fixed in the basilar memebrane of forward osmosis membrane, is effectively reduced and is just permeated
The interior concentration polarization of film.Forward osmosis membrane provided by the present invention has high permeating flux and efficient selective, and service life
Extend.
Description of the drawings
Transmission electron microscope figures of the Fig. 1 for allophane nano-tube.
Specific embodiment
The present invention using allophane nano-tube as modifying agent, pre-dispersed in casting solution, make during inversion of phases
Allophane nano-tube is stable in the presence of in film substrate, makes forward osmosis membrane possess higher permeability and selectivity, so as to drop
Low interior concentration polarization.The present invention is described in more detail by following examples and accompanying drawing, but the embodiment do not constitute right
The restriction of the present invention.
Embodiment 1
It is 4.5 by mass ratio：0.1：25 polysulfones, allophane nano-tube (as shown in Figure 1), N, N- dimethylacetamides
Amine mixes, first 30min under frequency 80KHz ultrasonic wave, then stirring and dissolving 6h uniformly solution, standing and defoaming at 80 DEG C
Casting solution is obtained after 12h, primary membrane is made by film forming is machining, enters 20 DEG C of quality percentages and contain after shaping in 10 minutes
Measure as 0.2%N, submergence 24h in the aqueous solution of N- dimethyl acetamides；It is 2% by gained basilar memebrane immersion weight/mass percentage composition
M-phenylene diamine (MPD) the aqueous solution in 1min, after draining the aqueous solution, transfer to the pyromellitic trimethylsilyl chloride that weight/mass percentage composition is 1%
Hexane solution in 1min, except striping excess surface solution after, film is heated 40min in 60 DEG C of baking ovens, allophane is obtained
Nano-tube hydridization polysulfones forward osmosis membrane.
Pure water flux of the basilar memebrane under 0.1MPa is determined using dead-end filtration method；Above-mentioned water aluminium is determined using contact angle instrument
The surface static contact angle of diamond stone nano-tube hydridization polysulfones forward osmosis membrane；With 2M NaCl solutions as liquid is drawn, with deionized water
For supplying liquid, its positive permeance property is evaluated.
Measurement result is：Under 0.1MPa pressure, the pure water flux of basilar memebrane is 28L m-2·h-1；Allophane silicon nanometer
The Static water contact angles of pipe hydridization polysulfones forward osmosis membrane are 96 °；25 DEG C, the water penetration flux of forward osmosis membrane is 1.65L m-2·
h-1, reverse flux salt is 1.07g m-2·h-1, structural parameters are 2411 μm.
Embodiment 2
It is 4.5 by mass ratio：0.2：25 polysulfones, allophane nano-tube, DMA mixing, first exist
30min under frequency 80KHz ultrasonic wave, then stirring and dissolving 6h uniformly solution at 80 DEG C, standing and defoaming is after 12 hours
To casting solution, primary membrane is made by film forming is machining, it is 0.2%N to enter weight/mass percentage composition after shaping in 10min,
Submergence 24h in the aqueous solution of N- dimethyl acetamides；Gained basilar memebrane is immersed the m-phenylene diamine (MPD) that weight/mass percentage composition is 2%
1min in the aqueous solution, after draining the aqueous solution, transfers in the hexane solution of the pyromellitic trimethylsilyl chloride that weight/mass percentage composition is 1%
1min, except striping excess surface solution after, film is heated 40min in 60 DEG C of baking ovens, allophane nano-tube hydridization is obtained
Polysulfones forward osmosis membrane.
Measurement result is：Under 0.1MPa pressure, the pure water flux of basilar memebrane is 94L m-2·h-1；Allophane silicon nanometer
The Static water contact angles that pipe hydridization PS membrane is just permeating are 87 °；25 DEG C, the water penetration flux of forward osmosis membrane is 5.18L m-2·
h-1, reverse flux salt is 11.06g m-2·h-1, structural parameters are 1714 μm.
Embodiment 3
It is 4.5 by mass ratio：0.3：25 polysulfones, allophane nano-tube, DMA mixing, first exist
30min under frequency 80KHz ultrasonic wave, then stirring and dissolving 6h uniformly solution at 80 DEG C, is cast after standing and defoaming 12h
Film liquid, makes primary membrane by film forming is machining, and it is 0.2%N, N- bis- to enter weight/mass percentage composition after shaping in 10min
Submergence 24h in the aqueous solution of methylacetamide；Gained basilar memebrane is immersed the water-soluble of the m-phenylene diamine (MPD) that weight/mass percentage composition is 2%
1min in liquid, after draining the aqueous solution, transfers in the hexane solution of the pyromellitic trimethylsilyl chloride that weight/mass percentage composition is 1%
1min, except striping excess surface solution after, film is heated 40min in 60 DEG C of baking ovens, allophane nano-tube hydridization is obtained
Polysulfones forward osmosis membrane.
Measurement result is：Under 0.1MPa pressure, the pure water flux of basilar memebrane is 193L m-2·h-1；Allophane silicon nanometer
The Static water contact angles of pipe hydridization polysulfones forward osmosis membrane are 73 °；25 DEG C, the water penetration flux of forward osmosis membrane is 5.79L m-2·
h-1, reverse flux salt is 2.71g m-2·h-1, structural parameters are 4234 μm.
Embodiment 4
It is 4.5 by mass ratio：0.9：25 polysulfones, allophane nano-tube, DMA mixing, first exist
30min under frequency 80KHz ultrasonic wave, then stirring and dissolving 6h uniformly solution at 80 DEG C, is cast after standing and defoaming 12h
Film liquid, makes primary membrane by film forming is machining, and it is 0.2%N, N- bis- to enter weight/mass percentage composition after shaping in 10min
Submergence 24h in the aqueous solution of methylacetamide；Gained basilar memebrane is immersed the water-soluble of the m-phenylene diamine (MPD) that weight/mass percentage composition is 2%
1min in liquid, after draining the aqueous solution, transfers in the hexane solution of the pyromellitic trimethylsilyl chloride that weight/mass percentage composition is 1%
1min, except striping excess surface solution after, film is heated 40min in 60 DEG C of water-baths, allophane nano-tube hydridization is obtained
Polysulfones forward osmosis membrane.
Measurement result is：Under 0.1MPa pressure, the pure water flux of basilar memebrane is 253L m-2·h-1；Allophane silicon nanometer
The Static water contact angles of pipe hydridization polysulfones forward osmosis membrane are 63 °；25 DEG C, the water penetration flux of forward osmosis membrane is 10.72L m-2·
h-1, reverse flux salt is 10.73g m-2·h-1, structural parameters are 2589 μm.
Comparative example 1
It is 4.5 by mass ratio：26 polysulfones, DMA mixing, then at 80 DEG C stirring and dissolving 6h into
Uniform solution, obtains casting solution, makes primary membrane by film forming is machining, after shaping in 10min after standing and defoaming 12h
Entrance weight/mass percentage composition is 0.2%N, submergence 24h in the aqueous solution of N- dimethyl acetamides；Gained basilar memebrane is immersed quality
Percentage composition be 2% m-phenylene diamine (MPD) the aqueous solution in 1min, after draining the aqueous solution, transfer to weight/mass percentage composition for 1%
Pyromellitic trimethylsilyl chloride hexane solution in 1min, except striping excess surface solution after, film is heated in 60 DEG C of baking ovens
40min, obtains Film laminated polysulfones forward osmosis membrane.
Measurement result is：Under 0.1MPa pressure, the pure water flux of basilar memebrane is 14L m-2·h-1；Pure polysulfones substrate is just oozed
The Static water contact angles of permeable membrane are 115 °；25 DEG C, the water penetration flux of forward osmosis membrane is 1.70L m-2·h-1, reverse flux salt
For 1.40g m-2·h-1, structural parameters are 5125 μm.
Relatively embodiment of the present invention 1-4 and comparative example 1 are visible, and the allophane nano-tube hydridization that the present invention is obtained just is oozed
The structural parameters of permeable membrane are significantly lower than the forward osmosis membrane with pure PS membrane as substrate, while after the former positive permeance property is better than
Person.For example, under the conditions of same test, the forward osmosis membrane of the optimum performance that the present invention is obtained do not increase in reverse flux salt or
On the premise of a small amount of growth, water penetration flux substantially increases 5L m-2·h-1More than.Thus explanation allophane nano-tube is miscellaneous
Change method can effectively reduce the interior concentration polarization of forward osmosis membrane, while improving water permeation performance and selecting performance.
Claims (9)
1. a kind of allophane nano-tube hydridization forward osmosis membrane, the allophane nano-tube hydridization forward osmosis membrane pass through with
Lower section method is prepared：
(1) allophane nano-tube, polymer, decentralized medium are mixed with organic solvent, ultrasonic wave disperses 5min～2h, plus
Thermal agitation forms uniform solution；In described casting solution, polymer, allophane nano-tube, the mass ratio of decentralized medium
For 10～30:0.01～3:1～4, and the mass percentage concentration of polymer is 15～35%, the quality of allophane nano-tube
Percentage concentration is 0.1～3%；Described ultrasonic frequency 20KHz～100KHz；Described heating stirring temperature is 40～80
DEG C, mixing time is 2～12h.
(2) casting solution is obtained after 10～24h of standing and defoaming, make primary membrane by film forming is machining.
(3) submergence about 10min～8h in coagulating bath is entered in about 5min after primary membrane shaping obtain basilar memebrane；Described coagulating bath
For deionized water or the aqueous solution of polar non-solute that weight/mass percentage composition is 0.1～60%；Described coagulation bath temperature
About 10～60 DEG C.
(4) further for basilar memebrane interfacial polymerization is formed aramid layer, obtains allophane nano-tube hydridization forward osmosis membrane, should
Step is specially：Basilar memebrane is immersed 0.1min～6min in the aqueous solution of polyamine, unnecessary polynary amine aqueous solution is removed, then
0.1min～6min in the organic solution of polynary acyl chlorides is immersed, unnecessary polynary solution of acid chloride is removed；After maturation process, tool is obtained
There is the allophane nano-tube hydridization forward osmosis membrane for cutting salt functional.The mass concentration of described polynary amine aqueous solution be 0.01～
1%；In the organic solution of described polynary acyl chlorides, the mass ratio of polynary acyl chlorides and organic solvent is 0.1～1:800～1000.
2. allophane nano-tube hydridization forward osmosis membrane according to claim 1, it is characterised in that described water aluminium English
Stone nano-tube is obtained in sodium orthosilicate and ANN aluminium nitrate nonahydrate synthesize by the following method：It is 0.58 by mol ratio:1 original
Sodium metasilicate and ANN aluminium nitrate nonahydrate are prepared into solution, and concentration is 0.1M NaOH adjusts the pH value of solution to 4.5～
5, reuse concentration for 0.1M hydrochloric acid by the pH of solution to adjusting to 4.3, after solution left standstill 2h, 95 DEG C are heated 3～7 days, room temperature
Cooling is stood, is that 0.1M ammonium hydroxide adjusts pH value to 8～9 with concentration, is formed gel, be centrifuged under 5000～9000rmp
10min～1h, obtains allophane nano-tube.
3. allophane nano-tube hydridization forward osmosis membrane according to claim 1, it is characterised in that described polymer
By the one kind in Kynoar, polyacrylonitrile, polysulfones, polyether sulfone, cellulose derivative, polyimides, polytetrafluoroethylene (PTFE) or
Multiple by any proportioning mixing composition；Described decentralized medium is mixed by any proportioning by one or more in water, ethanol, methyl alcohol
It is combined into；Described organic solvent is by dimethyl sulfoxide, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, crassitude
One or more in ketone is by any proportioning mixing composition.
4. allophane nano-tube hydridization forward osmosis membrane according to claim 1, it is characterised in that described coagulating bath
For the aqueous solution that weight/mass percentage composition is 10～30% polar non-solutes.
5. allophane nano-tube hydridization forward osmosis membrane according to claim 1, it is characterised in that described polyamine
By m-phenylene diamine (MPD), o-phenylenediamine, p-phenylenediamine, equal benzene triamine, piperazine and piperazine derivative one or more by arbitrarily matching somebody with somebody
Than mixing composition.
6. allophane nano-tube hydridization forward osmosis membrane according to claim 1, it is characterised in that described polynary acyl
Chlorine by pyromellitic trimethylsilyl chloride, m-phthaloyl chloride, o-phthaloyl chloride and paraphthaloyl chloride one or more by arbitrarily matching somebody with somebody
Than mixing composition.
7. allophane nano-tube hydridization forward osmosis membrane according to claim 1, it is characterised in that described polynary acyl
Organic solvent in the organic solution of chlorine is by the one kind in normal heptane, n-hexane, hexamethylene, naphthalene, Isopar-G and Isopar-E
Or it is several by any proportioning mixing composition.
8. allophane nano-tube hydridization forward osmosis membrane according to claim 1, it is characterised in that at described curing
Reason is specially：Composite membrane is put in 95 DEG C of water immersion 0.5min～5min, be put into after taking-up mass concentration for 0.1g/L～
0.1min～10min is soaked in the aqueous sodium hypochlorite solution of 1g/L, is put into mass concentration for the secondary of 0.1g/L～3g/L after taking-up
0.5min～10min is soaked in sodium chlorate aqueous solution；It is put into after taking-up in 95 DEG C of water and soaks 0.5min～5min or be put into
5min～40min is heated in 60～80 DEG C of baking oven.
9. allophane nano-tube hydridization forward osmosis membrane according to claim 1, it is characterised in that the non-matter of the polarity
Sub- solvent is by one or more in dimethyl sulfoxide, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, methyl pyrrolidone
By any proportioning mixing composition.
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| CN107866151A (en) * | 2017-11-03 | 2018-04-03 | 宁波大学 | A kind of one-dimensional compound forward osmosis membrane of single wall manosil AS nanotube |
| CN110302684A (en) * | 2019-04-18 | 2019-10-08 | 宁波大学 | Antipollution forward osmosis membrane based on amination manosil AS nanotube surface adsorption of modification |
| CN110756065A (en) * | 2019-10-30 | 2020-02-07 | 宁波大学 | Hydrotalcite-like nanosheet modified separation membrane, and preparation method and application thereof |
| CN112495195A (en) * | 2020-11-06 | 2021-03-16 | 大连理工大学 | Preparation method and application method of graphene oxide/carbon nanotube asymmetric separation membrane |
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